Distillation of solids



March 14,1939. K. c. D. HICKMAN DISTILLATION OF SOLIDS 2 Sheets-Sheet 1 Filed Feb. 21, 1936 INVENTOR.

Kenneth C. D. Hickman March 14, 1939- K. c. D. HICKMAN DISTILLATION OF SOLIDS Filed Feb. 21, 1956 2 Sheets-Shet 2 or; man .PM

' ATTO EYS mvm Kenneth C.D.Hik BY 4o moval on a commercial scale.

. Patented Mar. 14 ,1 93 9 v. I

UNITED STATES PATENT :OFFlCE DISTILIiATION or scans Kenneth C. D. Hickman, Rochester, N. Y., as-

signor, by mesne assignments, to Distillation Products, Inc., Rochester, N. Y., a corporation oi Delaware Application February 21, 1936, Serial No. 65,121 8 Claims. (01. 202-52) Thk invention relates to a process of high vacother object is to obtain concentrated distillates uum distillation and more particularly to the of oils such as glycerides, fat soluble vitamins, molecular distillation of solid mixtures and natsterols, etc., by subjecting natural solid materials wally-occurring products containing both solids containing them to molecular distillation. Other and liquids. objects will appear hereinafter. 5 Heretofore it has been customary to obtain oils These objects are accomplished by subjecting and extracts containing odors, drugs, vitamins, the solid materials to high vacuum distillation. and other principles from plant and vegetable It may be desirable to perform this distillation in substances and certain animal organs by subjecta number of stages, condensing part of the gases i0 ing the materials to high pressure. The liquid evolved at each stage in appropriately situated 10 which results from this treatment is only a portion a o e ch b s t p d that n of th t t l liquid contained in t material and t the final stage, the molecules of distillate shall be is usual t incl-ease the yield by p rformi g the allowed to have an appreciable, mean-free path expressing operation in a heated press or else by that the distillate can be condensed $111" adding solvent to h material before extraction, face located at a distance from the evaporative 15 No pressing process has yet succeeded in expellin surface of less than approximately the mean-free all the volatile or extractable substances from the fl material and while solvent extraction has enabled n he f ll w g examples and description I this to be done almost completely, it'entaiis a new have set forth several f e preferred embodiproblem, which is the elimination of the solvent ments 1 y invention, but it 15 t h un erstood 20 from the extract. Furthermore, it isnot possible that h y are incl de m r y for urp s of to choose any one solvent which will extract all illustration and not as a limitation thereof. the soluble or volatile substances from the origi- The Solid substance containing the de d'oi nal materiaL In the treatment of o11 be flng therapeutic agent, etc., is subject to distillation,

2:; seeds and of animal matter, containing fats and Pr y aft r mi ins and grinding. These oils, where the oil alone is of importance, the well 4 operations a e ry o b a up the ce lular known method of cold pressing yields an excellent Structure of o natural Pr cts a to leave product, the solid fibers of the vegetable and aniarge surface available for the m s on o mal matter providing a natural filtering mat a W le the m ncing and grinding i lw y for the purification of the oil. The greatest draw- P o d o distillation, t is on emplated 30' back to cold pressing is that the yield is lo that a further action of min ins and-grinding or A Hot pressing and solvent extraction increases the other action to di tu b yield, but they increase the contamination of the r e du th dis a o P es t elfoil with non-oily impurities, such as protein, Before the r li su j te to molecular sterols,.and odoriferous principles. 1 distillation, it is necessary to perform operations when, however, the oil is of secondary imporf degassing, d hydrating, a P lim n ry h h tance and the vitamin, sterol, and odoriferous or a um di i at on, t e vacuum. be n however,

medicinal constituents are of first importance, no not sufliciently high to be classed as molecular.

means hitherto known will efiect complete re- During each of these stages, the solids are pref- While hot pressing y p a over r e, heated surface. a It is and solvent extraction decrease the quantity of seldom practicable to leave the particles unconthe sterol, vitamins, or other accessory bodies left flned, owing to the tendency for individual grains in the matte, it isoften found that the concento explode and decrepitate. It is advantageous,

tration of these iactorsin the expressed oil is even therefore, to enclose the minced material in a less than secured by cold pressing, owing to dethin layer between -a lid surface and a porous 45 11 source material without recourse to expressing mo e rapidly 55 rent decomposition of the materials treated. An- T e m te l t b composition which occurs during the process. surface, or between two porous surfaces, and thus An object of this invention is to obtain the valthe materials t b di e may be ground a noble organic constituents such as oils, and therafed n the space b we n w r v li ands of peutic agents from solid animal and vegetable wire gauze. If one gauze is allowed to travel than the other, the imprisoned matent extraction o chemical t rial is continuously rolled and disturbed and newtreatment, solve Another object is to remove oils and therapeutic surfaces are exposed for the evolution of gas. may be heated by conduction or I agents such as vitamins from natural solid mate- The w gauze rials by high vacuum distillation without concurradiation or y eleotl'loltydistilled are finely chopped 5 the removal of substantially all volatllizable mat- Purification of the Figure 3 illustrates a vertical othe modification of Fig. 1 and;

Figure 4 illustrates a cross section taken on line 44 of Fig. 3.

Referring to of metal gauze, but which may be cloth or other fibrous material, supported by rolls III, II, I2, and I3, and driven by roll I4. Material to be distilled is placed in hopper I5 between endless belts I and 9. Vacuum chambers 3034 and distillation tilled solids leaving conveyor I at 8.

In Fig. 2 numeral 50 designates a rotatable distilled is introduced the the space between belt SI and cylinder 50 by hopper 69. per I0.

and 92 and rotating metering valves 93 and 94 respectively, the curved portions of partitions 9| and 92 making gas tight contact aided by lubricants if necessary, with rotating meteringdevices 93 and 94. Chambers 88 and 89 are maintained at a low pressure by vacuum casing 06 is maintained at a low pressure by a high vacuum pump, generally a condensation pump (not shown) connected to conduit I01.

Still casing I 08integral with .86 contains endless conveyor belt I09 disposed between cal rolls 0 and I II and is actuated by the latter.

I08 is evacuated by a high vacuum pump (not shown) connected to conduit I I 3. Distillate condensing on the inside walls of I08 flows by gravity into gutter I 00 and is removed through conduit II4. Scrapers Sand H6 are located in contact with belt conveyors 97 and I09 respectively and serve to remove adhering solids therefrom. Casing II I integral into gas tight Chamber H9 is I3I through which solid material is intermittently removed.

Referring to Figure 4 still casing 86 is shown integral with still'casing I08. Driving roll 98 for mounted on an Inside bearing I 34 and gas tight bearing I35. Shaft I31 mounted in bearings I38 mounted upon the inside walls I40 and I mounted and I 39'which are of still casing I08. Gutters Solid residue is withdrawn through hop-- I solid is introduced through the undue transfer of gas,

held at successively lower pressures pump Pi and auxil- .in Fig.

greater and greater di'iiiculty in penein passing through they find trating porous barriers and small apertures. It is the distilland to pass through narrow slits from compartment 39.. to 39bandso forth, without the successive compartments being due to the action oi. master iary pumps 32-5 which may be oi,-any convenient design appropriate for the pressure being handled.

The conveyor belts I and 9 are heated by electrical conduction and serve to raise the distllland to the required temperature. With most distillands much residual water is evolved in the early compartments of the still. With this water quantities of sterols, odoriierous materials and small amounts of vitamins are removed and may be collected in condensers 35 and 39. As the distilland penetrates the still, successively lower pressures are secured and in chamber 39 the pressure is so low that molecular distillation takes Master pump P1 will effect a reduction of pressure to about 400 mm. in 39,. and umps Pa, designed to produce successively lowerpressures so maintains a vacuum appropriate distillation. Pumps Ps-s operating in the sameto remove gases leaking through slits-from the exit end of the apparatus. are located at a distance from the distilland of less than about the mean free path and condensate collectingthereon flows by gravity into gutters 99 and thence to-withdrawal conduit 49. The distilland residue is then conveyed through chambers 39H into the atmosphere.

In some cases it may be desirable to enclose the distillation system of Fig. 1 in a gas tight vacuum casing and introduce and remove distilland using a hopper system such as disclosed 3. The amount of gas to be removed and. consequently the number of pumpsrequired would'be less. The expense and inconvenience of such a vacuum jacket confers doubtful advantages.

The conveyor belts I and the same speed but it has difierence in speed results in" stirring o! .the solid manner serve the successive 9mayberunat distilland andenables faster and more complete vaporization. The gauze used in the belt may have any desired aperture, but .a screen size considerably smaller than that of the distilland particles enables rapid removal of vapors and at the same through and filling the chambers.

In operating the apparatus of Fig.

aperture of 99 and forced or carried by belt through slit 59 into the distillation chamber where it is firmly held in a thin layer against the surface of. rotating cylinder 59 which is heated by electricity or circulation In chambers 64 and 65 degassing takes place at successively lower pressures maintained by pumps P1 and P: on the same principles explained in the description of Fig.1. Chamber 99 is maintained under a.

molecular vacuum andcondensate is condensed on walls oi casing 51 and withdrawn through an appropriately located conduitr Gas leaking through opening pump P5 and at a lower pressure in 91 by pump P4. Due to tensioning rolls 5! and 59 solids are tightly held against the walls of cylinder II.

thus possible to cause,

- rate of and degassed. Wheat germ germ and been found that a.

time prevents solids from sitting 2, powdered perature 59 is removed in chamber 69 by Solid residue is withdrawn through the aperture of hopper l9.

In the apparatus of Figs. 1 and 2 the number of degassing or pressure lowering chambers required to finally reach a molecular vacuum w1 depend upon thematerial treated, the design of the apparatus and the type, capacity and emciency of the pumps. It .is, therefore, to be understood that the type' of pumps and the number and size of vacuum chambers can be varied without departing from the spirit and scope of my invention.

In operation employing the apparatus of Figs. 3 and 4, solid, finely divided and dehydrated material to be distilled such as wheat germ is introduced into hopper 88 through opening 81 Hopper 98 should preferably be of sufficient capacity to hold enough material for a considerable period of operation without refilling. The wheat germ is then degassed by a vacuum pump connected with conduit 95'. This operation removes absorbed gases, residual water and volatile materials. The degassing rate can be increased by providing hopper 99' with heating means ,such as internal heating pipes. The wheat germ is conveyed into hopper 89 by rotating valve 93 the amount transferred being regulated by the size of its pocket. Valve 93 is in substantially gas tight contact with the curved portion of partition 9| and may be lubricated preferably with a dry lubricant such as graphite where contamination with a grease is undesirable. On entering hopper 99 the wheat germ is further degassed bya pump connectedwith conduit 96 andany gas entering through rotating valve 99 is also continuously re-' 89 is preferably of considerable volume in order to hold sufficient material to enable operation plate I99 at a rate controlled by therate of ro tation of valve 94 and is evenly distributed upon the conveyor belt 91 by the action of plates I99.

Conveyor belt 91 conveys the thinlayer of wheat germ over the heater I95 andasit is in contact therewith heat is transferred to the wheat it is thus raised to distilling temperature. The temperature may be so controlled that vitamin E alone or the vitamin and part or all of the glyceride content is vaporized. It is best to employ a temperature which vaporizes the vita-v min and part of the glycerides in still 86 and a temperature suilicient to vaporize the balance of glycerides in still I98. The vapors given off are condensed upon the inside walls of casing 86 and flowby gravity into gutters I49 and I (Fig. 4) and delivered thereby distillation A temand condensate is removed from the walls of I99 .by gutters mounted longitudinally thereon inthe same manner as in still casing 86 and delivered to conduit maintained in casing I98 by a high vacuum pump or pumps connecting with conduit H3. I f

The wheat germ falls by gravity from belt I99,

at the roll III, onto, partition I29 from which it is Wheat III. A high vacuum is transferred itohopper H9 by gas tight rotating valve I21 and thence into hopper.II9 through gas tight'rotating valve I29. Hopper I I9 is preferably -of sumc'ient volume to enable operation without frequent removal of distilland. Air entering on such removal is withdrawn by a pump connected with conduit I39 and gas 1 king past of residual gas.

valve I28 is removed. by a pump connected with conduit I29.

Casings 86 and cooled. ing fins or I08 are shown ey can be provided with jacketed for circulation of a cooling as being air to remove all H18 at a higher temperature. Obviously several still casings may be connected in series in order to remove any desired number of fractions.

ditions the distance separating the evaporating surface and the condensing surfaces 86 and I08 should be short and preferably should be less than about the mean free path of the molecules This distance varies according to the pressures obtaining in the stills.

When subjecting the soiids to what is known as molecular distillation the operating conditions distillation to take place. Processes of molecular distillation arethose occurring under such high vacuum conditions that a large proportion of the of less than approximately the mean free path of the molecules of residual gas. Greater distances may be employed, but only with considerable decrease in rate of tical purposes molecular distillation ceases where the distance is double the mean free path. The mean free path is inversely proportional to the of one inch may be used, or a quarter of an inch at less than 8 microns or ten inches at less than .3 micron, etc. With pressure and distance as micron or a distance of more than ten feet. Pressures greater than .1 mm. do not give a mean free path suflicient to separate the distillate without contamination.

ose below .01 mm. such as between .001 and .00001 mm. are preferred.

The process of plicable to conditions other than those used in molecular distillation procmses. The distance separating the evaporative and condensing surconvection.

In selecting the temperature to be used consideration must be given to distillation. For praction.

The process of my invention is applicable to the high vacuum distillation of any solid sub- What I claim is:

1. A method for tillation of solid disposing pieces of heated moving surface,

short-path, high vacuum dissubstances which comprises,

ized molecules on a near-by condensing surface and maintaining a high vacuum in the space between the surface of the layer and the condensing i surface.

3. The process of distilling pieces of chopped animal faces being maintained at .1 mm.

4. The process a pressure below about C. Vitamins can be satiswhereby the said are separated by a distance of less tance and by substantiallyunobstructed space, and maintaining a high vacuum in the space between the particles and the condensing surface compounds are volatilized and condensed upon the condensing surface.

5'. The process of removing and recovering, withoutharmful decomposition, complex, diflicultly volatilizable organic compounds from solid natural vegetable or animal substances that comprises mincing the substance into finely divided the particles, de-

discrete particles, degassing positing the degassed and finely divided particles in a thin layer, composed only of solid particles, on a heated movable conveyor, conveying them pasta condensing surface from which.the particles are separated by a short distance and'by substantially unobstructed space, and maintaining a high vacuum in the space between the particles and the condensing surface whereby the said compounds are volatilized and condensed upon the condensing surface.

6. The process of removing and recovering, without harmful decomposition, complex, difiicultly volatilizable organic compounds from solid natural vegetable or animal substances that comprises dividing the solid into small discrete particles, degassing gassed and finely divided particles in a thin layer, composed only of solid particles, on a heated movable conveyorfconveying them past a condensing surface from which the particles than approxi: mately ten inches and by substantially unobstructed space, and maintaining a pressure of less than approximately .1 mm. of mercury in the space between the particles and the condensing surface whereby the said compounds are the particles, depositing the devolatilized and condensed upon the condensing surface by high vacuum, short path distillation.

7. The process of removing and recovering without harmful decomposition a vegetable .or animal fat from solid vegetable or animal substances that comprises dividing the substance into small discrete particles, degassing the particles, depositing the degassed and finely divided particles in a thin layer, composed only of solid particles, on a heated movable conveyor, conveying them past a condensing surface from which the particles are separated by a distance of less than approximately the mean free path of the molecules of residual gas and maintaining a pressure of less than .1 mm. of mercury in the space between the particles and the condensing surface whereby the animal or vegetable fat is volatilized and condensed upon the condensing surface by molecular distillation.

8. The process of removing and recovering without harmful decomposition a vitamin from solid vegetable or animal substances that comprises dividing the'substance into small discrete particles, degassing the particles, depositing the degassed and finely divided particles in a thin layer, composed only of solid particles, on a heated movable conveyor, conveying them past a condensing surface are separated by a, distance of less than approximately the mean free path of residual gas and maintaining a pressure of less than .1 mm. of mercury in the space between the particles and the condensing surface whereby the vitamin is volatilized and condensed upon the condensing surface by molecular distillation.-

KENNETH o. D. HICKMANQ from which the particles 

